Fe2O3 nanoparticles (as maghemite and hematite mixtures) were prepared using adapted sol-gel method from a polyvinylpyrrolidone (PVP) aqueous solution in various Fe3+ : PVP monomer ratios. Analysis of X-ray diffraction was obtained to evaluate the crystalline state, average crystallite size, and composition of iron oxide phases. The morphology and average nanoparticles size were evaluated by electronic transmission microscopy. Magnetic properties of iron oxide were analyzed at low and room temperatures. Optical characteristics were evaluated by UV-Vis photoacoustic spectroscopy and the Mössbauer spectrum was obtained in order to evaluate subtle changes in the nuclear environment of the iron atoms.